The crystal structure of alicylaldehyde-4-piperidinothiosemicarbazone, , has been determined by single crystal X-ray analysis. The crystals are orthorhombic, space group , with unit cell dimensions a = 6.52(2), b = 13.42(4), c = 14.92(4). There are four formular units in a unit cell. The structure was solved by the heavy atom method and refined by isotropic block diagonal least-squares methods to a final R value of 0.10 for 1019 observed reflections. The oxygen atom of the hydroxyl group is involved in two hydrogen bonds, one as donor in the intramolecular O-HN hydrogen bond and the other as acceptor in the intermolecular N-HO hydrogen bond, the distances of the hydrogen bonds 2.56 and 3.00 respectively.The molecules are joined into infinite columns by the N-HO hydrogen bonds which form spirals along the two fold screw axis parallel to the a axis. The molecular columns are held together by van der Waals forces

The preferred conformation of benzenesulfenyl chloride was determined by EHMO calculation. It was found that the stability was dictated by the n- conjugation of S atom with the benzene ring. The ethanolysis reaction of benzenesulfenyl chlorides has been studied. The rate constants obtained have been discussed in terms of substituent effects and d-orbital participation of sulfur atom. From a non-linear Hammett plot, bipyramid type of intermediate has been suggested

The crystal structure of sodium sulfisoxazole hexahydrate, ,has been determined by X-ray diffraction method. The compound crystallizes in the monoclinic space group $$ with a = 15.68(3), b = 7.70(2), c = 17.94(4), = and Z = 4. A total of 1717 observed reflections were collected by the Weissenberg method with radiation. Structure was solved by heavy atom method and refined by block-diagonal least-squares methods to the R value of 0.14. The conformational angle formed by the S-C(l) bond with that of N(2)-C(7), when the projection in taken along the S-N(2), is The benzene ring is planar and makes an angle of with the plane of the isoxazole ring, which is also planar. The sodium atom has a distorted octahedral coordination of N(l) and five oxygen atoms from hydrate molecules. Sodium sulfisoxazole hexahydrate shows fourteen different hydrogen bondings in the crystal. These are six $O-H{\cdots}O-H bonds, three bonds, two one bond, with the distances in the range of 2.71 to

Amine salts of five tetrahedral and three octahedral oxalatoferrate(Ⅲ) complexes have been prepared including pyridinium salts of unreported oxalate complex ions and the latter being most photoreactive. The structural aspects of these new complex ions as well as of other oxalatoferrates(III) have been discussed based on their analytical data and infrared spectra. The results of molar conductivity and magnetic susceptibility measurements of all these oxalatoferrate(III) complexes were also presented

The determination of oxalic acid is carried out with Zr(IV)-XO complex by spectrophotometry. The Mechanism of this method in 1∼4N HCl solution is shown below (XO = xylenol orange); Zr(IV)+XO=Zr(IV)-XO+ excess XO, Zr(IV) - XO + oxalate = Zr(IV)-oxalate + XO When oxalic acid is added to Zr(IV)-XO complex(red color), the absorbance of Zr(IV) - XO complex is decreased in proportional to the amount of oxalic acid. The malic, malonic, maleic, fumaric, succinic, folic and glutamic acid did not interfere even if they are present in hundred times of oxalic acid. If they are present in the same amount as oxalic acid, citric and tartaric acid did not interfere but they are interfere when they are present in much more than that of oxalic acid

The rate constants of the derivatives of N-(2,4-dinitrophenyl)-benzimidoyl chloride were determined at various pH and a rate equation which can be applied over wide pH range was obtained. The reaction mechanism of hydrolysis of N-(2,4-dinitrophenyl)-benzimidoyl chloride which has not been studied carefully earlier in acidic and basic solution can be fullly explained by the rate equation obtained. The rate equation reveals that, beow pH 7.00, the hydrolysis of benzimidoyl chloride proceeds through reaction to form a carbonium ion intermediate.Above pH 8.5, however, the hydrolysis proceeds through the type reaction which depends on hydroxide ion and imidoyl chloride concentration. At pH 7.0∼8.5, two reactions occur competitively

A new mechanism is proposed for the reduction of nitrobenzene in basic solution that does not involve hydroxylamine as an intermediate. This paper presents evidence that the azoxybenzene is not formed from the hydroxylamine, but formed instead from the dimerization of nitrosobenzene

The addition of one mole of zinc chloride to 2.33 moles of sodium borohydride in tetrahydrofuran at room temperature gave a clear chloride-free supernatant solution of zinc borohydride after stirring three days and standing at room temperature.The approximate rates and stoichiometry of the reaction of zinc borohydride with 54 selected organic compounds were determined in order to test the utility of the reagent as a selective reducing agent. Aldehydes and ketones were reduced rapidly, aromatic ketones being somewhat slowly, and the double bond of cinnamaldehyde was not attacked. Acyl halides were reduced rapidly within one hour, but acid anhydrides were reduced at a moderate rate. Carboxylic acids, both aliphatic and aromatic, were slowly reduced to alcoholic stage. Esters were inert to this reagent but a cyclic ester, γ-butyrolactone, was slowly attacked. Primary amides were reduced slowly with partial evolution of hydrogen, whereas tertiary amides underwent neither reduction nor hydrogen evolution. Epoxides and nitriles were all inert, as well as nitro, azo, and azoxy compounds. Cyclohexanone oxime and phenyl isocyanate were reduced slowly but pyridine was inert. Disulfide, sulfoxide, sulfone and sulfonic acids were stable to this reagent

Four unreported derivatives of N-arylsulfonylbenzamide and six derivatives of N-arylsulfonylbenzimidothiophenyl ester were prepared. These were; p-methyl-N-(arylsulfonyl)benzamide, m-methyl-N-(arylsulfonyl)benzamide, m-nitro-N-(arylsulfonyl)benzamide, p-methoxy-N-(arylsulfonyl)benzamide, p-methyl-N-(arylsulfonyl)benzimidothiophenyl esters, p-chloro-N-(arylsulfonyl)benzimidothiophenyl ester, m-methyl-N-(arylsulfonyl)benzimidothiophenyl ester, p-nitro-N-(arylsulfonyl)benzimidothiophenyl ester, m-nitro-(arylsulfonyl)benzimidothiophenyl ester and p-methoxy-N-(arylsulfonyl)benzimidothiophenyl ester. The rate constants of the hydrolysis of N-arylsulfonylbenzimidothiophenyl esters were determined by ultraviolet spectrophotometry at various pH and rate equations which can be applied over a wide pH range were obtained. From the rate equation and substituent effects, one can conclude that above pH 11, the hydrolysis of N-arylsulfonylbenzimidothiophenyl esters are initiated by the attack of hydroxide ion, however, below pH 9, started by the addition of a water molecule on the azomethine group. At pH 9∼11, the competitive reaction between a water molecule and hydroxide ion is anticipated to occur